CN106744830B - A method of three-dimensional porous/two-dimensional slice graphene is prepared for carbon source with biology - Google Patents
A method of three-dimensional porous/two-dimensional slice graphene is prepared for carbon source with biology Download PDFInfo
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Abstract
The invention discloses a kind of methods for preparing three-dimensional porous/two-dimensional slice graphene as carbon source using biomass.The method steps are as follows: (1) biomass carbon source material being immersed in Fe (NO3)3·9H2In O solution；(2) the biomass carbon source material after immersion is calcined into carbonization, obtains Fe2O3/ C compound precursor；(3) by Fe2O3After/C compound precursor pickling, mixed under aqueous conditions with activator, it is dry；(4) desciccate is heat-treated；(5) heat-treated products are cleaned, it is dry, obtain three-dimensional porous/two-dimensional slice graphene.The advantages of the method for the present invention has experimentation simple, low in cost, environmental protection and energy saving.Three-dimensional porous graphene aperture prepared by the present invention is small, specific surface area is high；The two-dimensional slice graphene layer spacing of preparation is big, fault of construction is few, can be widely applied to include energy storage material, adsorbent material and Heat Conduction Material field.
Description
Technical field
The invention belongs to the preparation technical field of graphene, be related to it is a kind of using biomass as carbon source prepare it is three-dimensional porous/bis-
The method for tieing up Sheet Graphite alkene.
Background technique
Graphene is a kind of nano material haveing excellent performance with two-dimensional structure, has specific surface area high, and intensity is high, leads
The advantages that electrically strong.Currently, there are three types of the primary synthetic methods of graphene: hydro-thermal method, chemical vapour deposition technique and stripping method.Its
Although the graphene pore structure of middle hydro-thermal method preparation is relatively uniform, electric conductivity is not high, and preparation time is longer, limits it
Industrial application.The higher cost of chemical vapour deposition technique, and control condition is stringent, it is difficult to large-scale promotion production.Remove legal system
The yield of standby graphene is not high, and the graphene sheet layer agglomeration prepared is serious.
Summary of the invention
It is an object of the invention to solve production cost existing for existing three-dimensional porous/two-dimensional slice graphene preparation process
The problem of high, expensive, complex technical process, and one kind is provided and prepares three-dimensional porous/two-dimensional slice by carbon source of biomass
The method of graphene.
A method of three-dimensional porous/two-dimensional slice graphene being prepared by carbon source of biomass, specifically includes the following steps:
(1) biomass carbon source material is immersed in Fe (NO3)3·9H2In O solution；
(2) the biomass carbon source material after immersion is calcined into carbonization under inert gas atmosphere, obtains Fe2O3/ C compound
Precursor cleans in hydrochloric acid；
(3) Fe after cleaning2O3Activator is added in/C compound precursor, and is dissolved and is mixed with pure water, it is dry, it obtains
To intermediate product；
(4) obtained intermediate product is heat-treated in an inert gas atmosphere；
(5) product after being heat-treated is cleaned with hydrochloric acid, washes away metal and its oxide, then be washed with deionized water to cleaning solution
It is in neutrality, it is dry, obtain three-dimensional porous/two-dimensional slice graphene.
Preferably, in step (1), the biomass carbon source material includes agaric, and dry biomass carbon source material needs
It is soaked in Fe (NO again after impregnating expansion in deionized water3)3·9H2In O solution.
Preferably, in step (1), the time of the immersion is 18 ~ 20h.
Preferably, in step (1), the Fe (NO3)3·9H2The concentration of O solution is 0.5 ~ 3M.
Preferably, in step (2), the temperature of the calcining is 300 ~ 450 DEG C, and the time is 2 ~ 4h.
Preferably, in step (2), the biomass carbon source material after immersion is subjected to calcining carbonization again after drying.
Preferably, in step (2), the concentration of the hydrochloric acid is 0 ~ 6M.
Preferably, in step (2), the time of the cleaning is 20min ~ 6h, preferably 30 ~ 40min.
Preferably, in step (2), according to the difference of concentration of hydrochloric acid, three-dimensional porous or two-dimensional slice graphene is obtained；Work as step
Suddenly when concentration of hydrochloric acid is 0M in (2), three-dimensional porous graphene is obtained, when concentration of hydrochloric acid is between 0 ~ 6M in step (2), is obtained
To two-dimensional slice graphene.
Preferably, in step (3), the activator is potassium hydroxide, sodium hydroxide, calcium hydroxide, phosphoric acid, sulfuric acid and chlorine
Change one or more of zinc.
Preferably, in step (3), the additive amount of the activator are as follows: the mass ratio of biomass carbon source material and activator
For 1:1 ~ 5.
Preferably, in step (3), the drying is dry 1 ~ 5h under the conditions of 80 ~ 130 DEG C.
Preferably, in step (4), the heat treatment is first to be warming up to 300 ~ 400 DEG C with 5 ~ 10 DEG C/min of heating rate, is protected
0 ~ 1h of temperature；600 ~ 800 DEG C are warming up to 10 DEG C/min of heating rate again, is heat-treated 2 ~ 5h.
Preferably, in step (5), the drying is dry 0.5 ~ 5h under conditions of 40 ~ 100 DEG C.
Preferably, step (2), in (4), the inert gas is one or more of nitrogen, argon gas and helium.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) present invention synthesizes three-dimensional porous/two-dimensional slice graphene, preparation process letter by simple heat treatment method
Single, calcination temperature is low, and low energy consumption, meets environmental requirement.
(2) the biomass class carbon material of the invention to include agaric is carbon source, compared with the carbon source of other synthesizing graphite alkenes,
Have many advantages, such as that low toxicity, of low pollution, material is cheap and easy to get, raw material sources are extensive, low-carbon environment-friendly；It, will using this method and principle
Realize the more cheap three-dimensional porous and dilute large-scale production of two-dimensional slice graphite.
Detailed description of the invention
Fig. 1 is the XRD diagram of three-dimensional porous graphene prepared by embodiment 1；
Fig. 2 is the Raman spectrogram of three-dimensional porous graphene prepared by embodiment 1；
Fig. 3 is the SEM figure of three-dimensional porous graphene prepared by embodiment 1；
Fig. 4 is the SEM figure of three-dimensional porous graphene prepared by embodiment 1；
Fig. 5 is nitrogen adsorption-desorption figure of three-dimensional porous graphene prepared by embodiment 1；
Fig. 6 is the graph of pore diameter distribution of three-dimensional porous graphene prepared by embodiment 1；
Fig. 7 is the Raman spectrogram of two-dimensional slice graphene prepared by embodiment 3；
Fig. 8 is the SEM figure of two-dimensional slice graphene prepared by embodiment 3；
Fig. 9 is the SEM figure of two-dimensional slice graphene prepared by embodiment 3.
Specific embodiment
Below with reference to specific example, the present invention will be further described, but the present invention is not limited to following instances.
Embodiment 1
The preparation of three-dimensional porous graphene:
(1) dried fungus for weighing 10g is impregnated in deionized water, agaric water swelling after 20min, removes root
After be soaked in 3M Fe (NO3)3·9H2In O solution, agaric is placed in graphite crucible after 18h, covers, is placed in tube furnace,
300 DEG C of calcining 2h, obtain Fe in nitrogen atmosphere2O3/ C compound precursor；
(2) by Fe2O3The KOH of 5 times of quality is added in/C compound precursor stirring and washing 1h in 6M concentrated hydrochloric acid after cleaning
Solid and the mixing of 3mL deionized water dissolving, dry 2h under the conditions of 120 DEG C；Desciccate is placed in tube furnace, in nitrogen gas
Under atmosphere, 300 DEG C first are risen to the rate of 5 DEG C/min, 0h is kept the temperature, then rise to 700 DEG C with the rate of 10 DEG C/min, is heat-treated 3h；
Obtained sample is cleaned with 2M hydrochloric acid, and is washed with deionized water to cleaning solution and is in neutrality, and is finally dried in 60 DEG C of baking ovens
2h obtains three-dimensional porous graphene.
The X ray diffracting spectrum for the three-dimensional porous graphene that the present embodiment obtains is as shown in Figure 1, as shown in Figure 1, prepare
Three-dimensional porous graphene have diffraction maximum respectively at 21.5 °, 26.3 ° and 44.6 °, wherein 21.5 ° and 44.6 ° of diffraction maximum explanation
Material is graphene-structured, and according to 21.5 ° of diffraction maximum, can be calculated the stacking interlayer of graphene in conjunction with Bragg equation
Away from for 0.41nm；And the weak peak at 26.3 ° illustrates in material still with the presence of the micro graphite not being fully exfoliated.
The Raman spectrogram for the three-dimensional porous graphene that the present embodiment obtains is as shown in Figure 2, it can be seen that Raman spectrogram
Middle there are apparent characteristic peaks at three: the peak D (1350cm-1), the peak G (1593cm-1) and the peak 2D (2823cm-1).It is fitted by swarming
And it is 1.36 that Id/Ig, which is calculated, illustrates that the degree of graphitization of resulting materials is higher.
Such as Fig. 3 of the scanning electron microscope analysis under different multiples for the three-dimensional porous graphene that the present embodiment obtains and
Shown in Fig. 4, as seen from the figure, the three-dimensional grapheme of preparation is perforated grill structure.
The nitrogen adsorption for the three-dimensional porous graphene that the present embodiment obtains-desorption figure is as shown in figure 5, as can be seen from the figure
Prepared three-dimensional porous graphene specific surface area with higher, about 507cm3/g。
The graph of pore diameter distribution for the three-dimensional porous graphene that the present embodiment obtains is as shown in fig. 6, three-dimensional more as can be seen from Figure
Hole graphene is largely microcellular structure, and pore size is in 3nm or less.
Embodiment 2
The preparation of three-dimensional porous graphene:
(1) dried fungus for weighing 10g is impregnated in deionized water, agaric water swelling after 20min, removes root
After be soaked in 0.5M Fe (NO3)3·9H2In O solution, agaric is placed in culture dish after 20h, is placed in refrigerator and freezes 12h, is put
Enter in vacuum freeze drier and is freeze-dried for 24 hours；Agaric after freeze-drying is put into graphite crucible, covers, is placed in tubular type
In furnace, 450 DEG C of calcining 4h, obtain Fe in nitrogen atmosphere2O3/ C compound precursor；
(2) by Fe2O31 times of quality is added in/C compound precursor stirring and washing 6h in 0.001M dilute hydrochloric acid after cleaning
KOH solid and the mixing of 3mL deionized water dissolving, dry 5h under the conditions of 80 DEG C；Drying is placed in tube furnace, in argon atmosphere
Under, 400 DEG C first are risen to the rate of 10 DEG C/min, 1h is kept the temperature, then rise to 800 DEG C with the rate of 10 DEG C/min, is heat-treated 2h；?
To sample cleaned with 2M hydrochloric acid, and be washed with deionized water to cleaning solution and be in neutrality, finally dry 5h in 40 DEG C of baking ovens,
Obtain three-dimensional porous graphene.
Obtained three-dimensional porous graphite is similar to three-dimensional porous graphene prepared by embodiment 1, is perforated grill structure, tool
There is high specific surface area, pore size is in 3nm or less.
Embodiment 3
The preparation of two-dimensional slice graphene:
(1) dried fungus for weighing 10g is impregnated in deionized water, agaric water swelling after 20min, removes root
After be soaked in 2M Fe (NO3)3·9H2In O solution, agaric is placed in graphite crucible after 19h, covers, is placed in tube furnace,
425 DEG C of calcining 3h, obtain Fe in nitrogen atmosphere2O3/ C compound precursor；
(2) by Fe2O3/ C compound precursor cleans 20min in pure water, and the KOH solid and 3mL of 4 times of quality are added afterwards
Deionized water dissolving mixing, dry 1h under the conditions of 130 DEG C；Desciccate is placed in tube furnace, in a nitrogen atmosphere, first with
The rate of 7 DEG C/min rises to 350 DEG C, keeps the temperature 0.5h, then rise to 600 DEG C with the rate of 10 DEG C/min, is heat-treated 5h；Obtained sample
Product are cleaned with 2M hydrochloric acid, and are washed with deionized water to cleaning solution and are in neutrality, and are finally dried 0.5h in 100 DEG C of baking ovens, are obtained
To two-dimensional slice graphene.
The Raman spectrogram for the two-dimensional slice graphene that the present embodiment obtains is as shown in Figure 7, it can be seen that Raman spectrogram
Middle there are apparent characteristic peaks at three: the peak D (1344cm-1), the peak G (1574cm-1) and the peak 2D (2718cm-1).It is fitted by swarming
Know that the peak 2D is single Lorentz fit peak, peak position (2700cm of the peak position compared with single-layer graphene-1) blue shift, explanation is not single layer
Graphene；And IG/I2D=0.88, illustrate the number of plies of graphene less than 5.
Such as Fig. 8 of the scanning electron microscope analysis under different multiples for the two-dimensional slice graphene that the present embodiment obtains and
Shown in 9, as seen from the figure, the two-dimensional graphene of preparation is lamellar structure, and piece interlamellar spacing is larger, and lamella is very thin.
Claims (9)
1. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass, which comprises the steps of:
(1) biomass carbon source material is immersed in Fe (NO3)3·9H2In O solution；
(2) the biomass carbon source material after immersion is calcined into carbonization under an inert atmosphere, obtains Fe2O3/ C compound precursor, then
Yu Shuizhong cleaning；
(3) Fe after cleaning2O3It is added activator in/C compound precursor, and is dissolved and mixed with pure water, it is dry, it obtains
Between product；
(4) obtained intermediate product is heat-treated in an inert gas atmosphere；
(5) product after being heat-treated is cleaned with hydrochloric acid, washes away metal and its oxide, then is washed with deionized water to cleaning solution and is in
Property, it is dry, obtain two-dimensional slice graphene.
2. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (1), the biomass carbon source material includes agaric, and dry biomass carbon source material needs to soak in deionized water
Then at Fe (NO after bubble expansion3)3·9H218 ~ 20h is impregnated in O solution；Fe (the NO3)3·9H2The concentration of O solution be 0.5 ~
3M。
3. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (2), the temperature of the calcining is 300 ~ 450 DEG C, and the time is 2 ~ 4h；The time of the cleaning is 20min ~ 6h.
4. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (2), the biomass carbon source material after immersion is carried out calcining carbonization again after drying.
5. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In the time of cleaning described in step (2) is 30 ~ 40min.
6. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (3), the activator is one of potassium hydroxide, sodium hydroxide, calcium hydroxide, phosphoric acid, sulfuric acid and zinc chloride
More than, the mass ratio of biomass carbon source material and activator is 1:1 ~ 5；The drying be dry 1 under the conditions of 80 ~ 130 DEG C ~
5h。
7. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (4), the heat treatment is first to be warming up to 300 ~ 400 DEG C with 5 ~ 10 DEG C/min of heating rate, keeps the temperature 0 ~ 1h；Again with
10 DEG C/min of heating rate is warming up to 600 ~ 800 DEG C, is heat-treated 2 ~ 5h.
8. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (5), the drying is dry 0.5 ~ 5h under conditions of 40 ~ 100 DEG C.
9. a kind of method for preparing two-dimensional slice graphene as carbon source using biomass according to claim 1, feature exist
In in step (2), (4), the inert atmosphere is one or more of nitrogen, argon gas and helium.
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| CN109399615B (en) * | 2018-11-27 | 2022-06-07 | 天津科技大学 | Preparation method of 3D-graphene material with biomass resource as carbon source |
| CN109939643A (en) * | 2019-04-09 | 2019-06-28 | 西安工业大学 | α-Fe2O3Adulterate the preparation method and applications of charcoal |
| CN110395723B (en) * | 2019-08-26 | 2021-06-01 | 东莞理工学院 | Method for preparing high-performance graphene by molten salt strategy |
| CN113429933A (en) * | 2021-07-30 | 2021-09-24 | 陕西科技大学 | Ferroferric oxide/biomass porous carbon composite wave-absorbing material and preparation method thereof |
| CN114261955B (en) * | 2021-12-03 | 2024-01-30 | 海南师范大学 | Gelidium amansii derived tri-carbon tetranitride/porous graphitized carbon as well as preparation method and application thereof |
| CN115557490A (en) * | 2022-10-18 | 2023-01-03 | 武汉工程大学 | Method for preparing biomass-based vertical graphene in batches |
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